CN101824238A - Surface treatment method for powder composition of optical diffusion plastic - Google Patents
Surface treatment method for powder composition of optical diffusion plastic Download PDFInfo
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Abstract
The invention relates to a surface treatment method for a powder composition of optical diffusion plastic, which is characterized by comprising the following steps: modifying the surfaces of inorganic optical diffusion particles with a silane coupling agent in an in-situ polymerization method, ultrasonically dispersing the inorganic optical diffusion particles into an organic solvent, and slowly dripping mixed solution of an initiator and (methyl) acrylic acid and ester monomers thereof at a certain temperature for polymerization, thereby obtaining the product. Since the compound with the core-shell structure is prepared through in-situ realization and combination of the inorganic particles, the invention not only improves the compatibility of the powder composition and the transparent plastic substrate, but also has no large changes in optical properties. Moreover, the refractive index matching degree of the powder composition and the transparent plastic substrate can be effectively adjusted through changing the thickness of the shell layer and the core layer of the powder composition, thereby realizing high transparency and optical diffusibility.
Description
Technical field
The present invention relates to a kind of surface treatment method that is used for the powder composition of optical diffusion plastic.
Background technology
Along with the liquid-crystal display that develops rapidly of communication and household electric appliances is attracted attention day by day, domestic manufacturers drop into the research and development of liquid-crystal display related industries in succession.Liquid-crystal display is compared with other indicating system, not only has outside the advantages such as volume is little, in light weight, also has the feature of low power consumption and low operating voltage, and has color and show diversified possibility.Module backlight in the liquid-crystal display generally comprises parts such as light source, reflector, light guiding plate, diffuser plate and light collecting plate, and wherein the function of diffuser plate is to provide a uniform surface light source for liquid-crystal display.The generation of light flooding mechanism at present mainly is by surface tissue and the inner diffusion particle dual mode of filling, and wherein most of novel photodiffusion materials are transparent polymer matrix and diffusant particle blend preparation.Particulate as light diffusing agent is mainly inorganic nano-particle, and as materials such as glass microballon, silicon-dioxide, the particle diameter of these inorganic nano-particles is very little, surface-area is bigger, reunite easily, and and the consistency of transparent polymer matrix relatively poor, thereby influence the transmittance of photodiffusion material.In addition since the specific refractory power of transparent polymer material and the specific refractory power of inorganic nano-filler generally all do not match, inevitably all there is the scattering of light effect in prepared inorganic nano-particle/polymer composite, and very difficult preparation has the inorganic nano-particle/polymer composite of high transparent.
At the composite particles of inorganic nano-particle sub-surface coated high molecular formation nucleocapsid structure, can change the performances such as light, magnetic, heat, electric property and surfactivity of inorganic nano-particle.If inorganic light diffusing agent is carried out surface treatment, it is compound to carry out in-situ polymerization with (methyl) vinylformic acid and ester compound thereof, form certain thickness shell, be prepared into composite particles with nucleocapsid structure, reach the purpose of regulating the material specific refractory power by regulating each components contents of nucleocapsid, this just might make the polymer-based photodiffusion material with high transparent essentially.
The nucleocapsid structure compound is used widely in sizing agent, coating and polymer matrix composite field.Chinese invention patent 200610016261.8 has been reported poly acrylate composite emulsion and the methods for making and using same thereof that a kind of pressure-sensitive adhesive agent is used, the latex particle of forming this composite emulsion is nuclear with the surface through silane coupler modified nano silicon, multipolymer with acrylate and Acrylic Acid Monomer is a shell, nano silicon is uniformly dispersed in the polyacrylate pressure-sensitive matrix, and latex particle shell and shell thickness can be controlled.Patent 200910020490.0 has been reported a kind of preparation method of single distributed nuclei shell structured composite nano particle, is nuclear with the nano silicon, prepares the good silicon-dioxide of monodispersity/high polymer composite nano particle by semicontinuous emulsifier-free emulsion polymerization.These all are by method of emulsion polymerization, and additive such as emulsifying agent, tensio-active agent is difficult to remove in the reaction system, remain in the optical property that can influence final product in the system.Utilizing in-situ polymerization is the method for preparing the more easy easier realization industrialization of nucleocapsid structure compound.Have report to adopt the interface in-situ polymerization, preparation is a nuclear with the calcium sulfate particle, and methyl methacrylate is that the nucleocapsid structure compound of shell is used for polyvinyl chloride composite materials and has better dispersiveness (New Chemical Materials, 2008,36 (1): 77); With methacrylic acid nano-silica surface is carried out the lipophilicity (applied chemistry, 2003, (20) 10:1003) that the in-situ polymerization modification can improve nano silicon; Azo dicyano valeric acid is incorporated into the nano-calcium carbonate surface, causes the methyl methacrylate heterogeneous polymerization, in the polymerization process, particle aggregation is known from experience peeling off to a certain degree, and size of particles reduces (chemical reaction engineering and technology, 2005,21 (3): 234).But the method for utilizing in-situ polymerization is used for the optical diffusion plastic field with poly-(methyl) vinylformic acid and ester compound coated inorganic light diffusion particle thereof and yet there are no report.
Summary of the invention
The objective of the invention is in order to solve above technical problem, a kind of surface treatment method that is used for the powder composition of optical diffusion plastic is provided, said composition is compared than other light diffusing agent compositions, and has better consistency and optical property after the blend of transparent plastics matrix.
The technical scheme that the present invention takes is to adopt the method for in-situ polymerization, after earlier inorganic smooth diffusion particle being used the silane coupling agent surface modification, ultra-sonic dispersion is in organic solvent, at a certain temperature, the mixing solutions polymerization that slowly drips initiator and (methyl) vinylformic acid and esters monomer thereof obtains product.The compound compound with nucleocapsid structure that makes of in-situ accomplishes and inorganic particulate, when improving powder composition and transparent plastics matrix consistency, optical property changes little.
The silane coupling agent that is used for inorganic light diffusing agent improving particle surface among the present invention is at least a of vinyl silanes, aminosilane, methacryloxy silane.Concrete steps for the inorganic light diffusing agent particle of certain mass in 100 ℃ of high speed agitators with the powder quality mark be 1～5% silane coupler modified, powder is packed in the organic solvents such as butanone, toluene after the modification, ultra-sonic dispersion 30min～2h slowly drips (methyl) vinylformic acid prepare in advance and the mixing solutions of esters monomer and initiator thereof again.Temperature is controlled at about 60～90 ℃, reaction 2～5h, and making with inorganic light diffusing agent particle is nuclear, poly-(methyl) vinylformic acid and ester compound thereof are the core-shell particles structure of shell.Wherein initiator is a kind of in peroxide initiator and the azo-compound initiator.
(methyl) vinylformic acid of the present invention and ester compound thereof are at least a in (methyl) vinylformic acid, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) glycidyl acrylate, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, (methyl) 2-EHA.
Inorganic light diffusing agent particle of the present invention is at least a in silicon-dioxide, aluminum oxide, magnesium oxide, lime carbonate, barium sulfate, the glass microballon.
Transparent plastics matrix of the present invention is at least a in polymethylmethacrylate, polycarbonate, polystyrene, polypropylene, copolymer of methyl methacrylatestyrene, maleic anhydride-styrene copolymers, methyl methacrylate-acrylate copolymer, the poly-cycloolefin.
In order to realize the high transparent of optical diffusion plastic, the absolute value of the index difference of powder composition of the present invention and transparent plastics matrix is 0.05 or more.The weight percent of described powder composition and transparent plastics matrix is 1/2000～1/10.The particle diameter of mineral compound is 0.5～20 μ m in the described powder composition.The polymer shell layer thickness that is used for the coated inorganic compound in the described powder composition is 0.5～15 μ m.
Embodiment
Further specify the present invention below by embodiment, therefore do not limit the present invention among the described scope of embodiments.
Embodiment 1
The calcium carbonate powder of certain mass adds the YDH-151 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of butanone solvent, and ultrasonic dispersing 30min, slowly drip the methyl methacrylate prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the calcium carbonate particles is nuclear, polymethylmethacrylate is the core-shell particles structure of shell.
With weight percent 4% be nuclear with lime carbonate, polymethylmethacrylate is that the polycarbonate of light diffusing agent (particle diameter is 10 μ m, polymethyl methacrylate shells layer thickness 0.7 μ m), weight percent 96% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusing polycarbonate composition transmittance that 2mm is thick is 80.1%, and mist degree is 90.2%.
Embodiment 2
With the KH-550 silane coupling agent to nanometer SiO
2Surface modification, agitator, N are being housed
2In the four-hole boiling flask of gas ingress pipe, prolong, thermometer, feed N
2Gas adds toluene 100mL, is warming up to boiling, adds 2g SiO
2(use preceding 100 ℃ handle 12h) adds the silane coupling agent 5mL of hydrolysis, stirs, and refluxes, react behind 4 h reaction product.Get the SiO after the modification
2Be scattered in the toluene solution of 100mL, feed N
2Gas stirs, and is warming up to 80 ℃ gradually, adds the initiator benzoyl peroxide, dropwise drips methacrylic acid, 0.5mL/min, and reaction 3h gets product.
With weight percent 2% is nuclear with silicon-dioxide, polymethyl acrylic acid is that the polymethylmethacrylate of light scattering agent (particle diameter is 12 μ m, polymethyl methacrylate shells layer thickness 0.8 μ m), weight percent 98% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusion polymethylmethacrylacomposition composition transmittance that 2mm is thick is 78.3%, and mist degree is 89.2%.
Embodiment 3
The barium sulfate powder of certain mass adds the YDH-151 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of butanone solvent, and ultrasonic dispersing 30min, slowly drip the glycidyl methacrylate prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the barium sulfate particle is nuclear, poly (glycidyl methacrylate) is the core-shell particles structure of shell.
With weight percent 3% is nuclear with barium sulfate, poly (glycidyl methacrylate) is that the polycarbonate of light diffusing agent (particle diameter is 10 μ m, poly (glycidyl methacrylate) shell thickness 0.7 μ m), weight percent 97% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusing polycarbonate composition transmittance that 2mm is thick is 79.2%, and mist degree is 89.1%.
Embodiment 4
The glass microballon powder of certain mass adds the KH-560 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of butanone solvent, and ultrasonic dispersing 30min, slowly drip the Jia Jibingxisuanyizhi prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the glass microballon particle is nuclear, polyethyl methacrylate is the core-shell particles structure of shell.
With weight percent 3% be nuclear with the glass microballon, polyethyl methacrylate is that the polystyrene of light diffusing agent (particle diameter is 8 μ m, polyethyl methacrylate shell thickness 0.5 μ m), weight percent 97% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusion polyphenylacetylene combination transmittance that 2mm is thick is 77.4%, and mist degree is 88.3%.
Embodiment 5
Certain mass alumina powder jointed adds the KH-570 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of butanone solvent, and ultrasonic dispersing 30min, slowly drip the Hydroxyethyl acrylate prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the aluminium oxide particles is nuclear, Poly(Hydroxyethyl Methacrylate) is the core-shell particles structure of shell.
With weight percent 2% be nuclear with the aluminum oxide, Poly(Hydroxyethyl Methacrylate) is that the polypropylene of light diffusing agent (particle diameter is 12 μ m, Poly(Hydroxyethyl Methacrylate) shell thickness 0.6 μ m), weight percent 98% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusion polypropene composition transmittance that 2mm is thick is 75.6%, and mist degree is 84.7%.
Embodiment 6
The magnesium oxide powder of certain mass adds the KH-550 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of toluene solvant, and ultrasonic dispersing 30min, slowly drip the methacrylic acid 2-ethylhexyl prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the magnesia particle is nuclear, polymethyl acrylic acid 2-ethylhexyl is the core-shell particles structure of shell.
With weight percent 2% is nuclear with magnesium oxide, polymethyl acrylic acid 2-ethylhexyl is that the polymethylmethacrylate-styrol copolymer of light diffusing agent (particle diameter is 11 μ m, polymethyl acrylic acid 2-ethylhexyl shell thickness 0.4 μ m), weight percent 98% of shell is through the twin screw extruder extrusion compositions.Through measuring, light diffusion polymethylmethacrylate-styrene copolymer composite transmittance that 2mm is thick is 79.8%, and mist degree is 90.7%.
Embodiment 7
The silicon-dioxide powdery of certain mass adds the A-171 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of toluene solvant, and ultrasonic dispersing 30min, slowly drip the butyl acrylate prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the silicon dioxide granule is nuclear, butyl polyacrylate is the core-shell particles structure of shell.Refractive index difference through measuring this core-shell particles and polycarbonate is 0.05.
With weight percent 3% be nuclear with silicon-dioxide, butyl polyacrylate is that the polycarbonate of light diffusing agent (particle diameter is 7 μ m, butyl polyacrylate shell thickness 0.5 μ m), weight percent 97% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusing polycarbonate composition transmittance that 2mm is thick is 81.6%, and mist degree is 92.3%.
Embodiment 8
The silicon-dioxide powdery of certain mass adds the A-174 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of toluene solvant, and ultrasonic dispersing 30min, slowly drip the Rocryl 410 prepare in advance and the mixing solutions of benzoyl peroxide again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the silicon dioxide granule is nuclear, the polymethyl acrylic acid hydroxypropyl acrylate is the core-shell particles structure of shell.
With weight percent 4% is nuclear with silicon-dioxide, the polymethyl acrylic acid hydroxypropyl acrylate is that the polycarbonate of light diffusing agent (particle diameter is 8 μ m, polymethyl acrylic acid hydroxypropyl acrylate shell thickness 0.5 μ m), weight percent 96% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusing polycarbonate composition transmittance that 2mm is thick is 80.2%, and mist degree is 91.4%.
Embodiment 9
The calcium carbonate powder of certain mass adds the A-174 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of butanone solvent, and ultrasonic dispersing 60min, slowly drip the butyl methacrylate prepare in advance and the mixing solutions of benzoyl peroxide again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the calcium carbonate particles is nuclear, poly-n-butyl methacrylate is the core-shell particles structure of shell.
With weight percent 5% is nuclear with lime carbonate, poly-n-butyl methacrylate is that the methyl methacrylate-acrylate copolymer of light diffusing agent (particle diameter is 8 μ m, poly-n-butyl methacrylate shell thickness 0.5 μ m), weight percent 95% of shell is through the twin screw extruder extrusion compositions.Through measuring, light diffusion methyl methacrylate-acrylic acid ester copolymer composition transmittance that 2mm is thick is 79.3%, and mist degree is 89.6%.
Embodiment 10
The silicon-dioxide powdery of certain mass adds the A-174 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of toluene solvant, and ultrasonic dispersing 60min, slowly drip the vinylformic acid prepare in advance and the mixing solutions of benzoyl peroxide again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the silicon dioxide granule is nuclear, polyacrylic acid is the core-shell particles structure of shell.
With weight percent 5% be nuclear with silicon-dioxide, polyacrylic acid is that the maleic anhydride-styrene copolymers of light diffusing agent (particle diameter is 8 μ m, polyacrylic acid shell thickness 0.5 μ m), weight percent 95% of shell is through the twin screw extruder extrusion compositions.Through measuring, the light diffusion maleic anhydride-styrene copolymers composition transmittance that 2mm is thick is 80.5%, and mist degree is 91.7%.
Embodiment 11
The barium sulfate powder of certain mass adds the KH-560 of powder quality 1.5% in 100 ℃ of high speed agitators silane coupler modified, powder adding after the modification is equipped with in the there-necked flask of toluene solvant, and ultrasonic dispersing 30min, slowly drip the ethyl propenoate prepare in advance and the mixing solutions of Diisopropyl azodicarboxylate again.Temperature is controlled at about 80 ℃, the reaction 3h, after be warming up to 90 ℃, discharging behind the 30min, making with the barium sulfate particle is nuclear, polyethyl acrylate is the core-shell particles structure of shell, the refractive index difference through measuring this core-shell particles and poly-cycloolefin is 0.1.
With weight percent 3% be nuclear with barium sulfate, polyethyl acrylate is that the poly-cycloolefin of light diffusing agent (particle diameter is 6 μ m, polyethyl acrylate shell thickness 0.8 μ m), weight percent 97% of shell is through the twin screw extruder extrusion compositions.Through measuring, the poly-cycloolefin composition transmittance of light diffusion that 2mm is thick is 78.4%, and mist degree is 88.6%.
Claims (10)
1. surface treatment method that is used for the powder composition of optical diffusion plastic, it is characterized in that adopting the method for in-situ polymerization, after earlier inorganic smooth diffusion particle being used the silane coupling agent surface modification, ultra-sonic dispersion slowly drips initiator and (methyl) vinylformic acid and the polymerization of esters monomer mixing solutions thereof at a certain temperature and obtains product in organic solvent.The compound compound with nucleocapsid structure that makes of in-situ accomplishes and inorganic particulate, when improving powder composition and transparent plastics matrix consistency, optical property changes little.
2. composition according to claim 1 is characterized in that: described silane coupling agent is at least a in vinyl silanes, aminosilane, the methacryloxy silane.
3. composition according to claim 1 is characterized in that: described initiator is a kind of in peroxide initiator and the azo-compound initiator.
4. composition according to claim 1 is characterized in that: described (methyl) vinylformic acid and ester compound thereof are at least a in (methyl) vinylformic acid, (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) butyl acrylate, (methyl) glycidyl acrylate, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, (methyl) 2-EHA.
5. composition according to claim 1 is characterized in that: described inorganic smooth diffusion particle is a kind of in silicon-dioxide, aluminum oxide, magnesium oxide, lime carbonate, barium sulfate, the glass microballon.
6. composition according to claim 1 is characterized in that: described transparent plastics matrix is a kind of in polymethylmethacrylate, polycarbonate, polystyrene, polypropylene, copolymer of methyl methacrylatestyrene, maleic anhydride-styrene copolymers, methyl methacrylate-acrylate copolymer, the poly-cycloolefin.
7. composition according to claim 1 is characterized in that: the absolute value of the index difference of described powder composition and transparent plastics matrix is smaller or equal to 0.1.
8. composition according to claim 1 is characterized in that: the weight percent of described powder composition and transparent plastics matrix is 1/2000～1/10.
9. composition according to claim 1 is characterized in that: the particle diameter of mineral compound is 0.5～20 μ m in the described powder composition.
10. composition according to claim 1 is characterized in that: the polymer shell layer thickness that is used for the coated inorganic compound in the described powder composition is 0.5～15 μ m.
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